EP0037321B1 - Procédé de préparation de matériaux adsorbants destinés à l'analyse ou au traitement des liquides et les matériaux ainsi obtenus - Google Patents
Procédé de préparation de matériaux adsorbants destinés à l'analyse ou au traitement des liquides et les matériaux ainsi obtenus Download PDFInfo
- Publication number
- EP0037321B1 EP0037321B1 EP81400456A EP81400456A EP0037321B1 EP 0037321 B1 EP0037321 B1 EP 0037321B1 EP 81400456 A EP81400456 A EP 81400456A EP 81400456 A EP81400456 A EP 81400456A EP 0037321 B1 EP0037321 B1 EP 0037321B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- adsorbent
- alkali metal
- heat treatment
- conducted
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 239000003463 adsorbent Substances 0.000 title claims description 71
- 239000000463 material Substances 0.000 title claims description 49
- 238000000034 method Methods 0.000 title claims description 19
- 239000007788 liquid Substances 0.000 title claims description 4
- 239000000243 solution Substances 0.000 claims description 30
- 239000000126 substance Substances 0.000 claims description 29
- 238000010438 heat treatment Methods 0.000 claims description 26
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 10
- 239000011707 mineral Substances 0.000 claims description 10
- 229910052783 alkali metal Inorganic materials 0.000 claims description 9
- 150000001340 alkali metals Chemical class 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 8
- 229910052910 alkali metal silicate Inorganic materials 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical class [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims 1
- 235000011114 ammonium hydroxide Nutrition 0.000 claims 1
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 230000001105 regulatory effect Effects 0.000 claims 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 48
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 12
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical group O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 12
- MSNWSDPPULHLDL-UHFFFAOYSA-K ferric hydroxide Chemical compound [OH-].[OH-].[OH-].[Fe+3] MSNWSDPPULHLDL-UHFFFAOYSA-K 0.000 description 7
- 239000004115 Sodium Silicate Substances 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 6
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 6
- 229910052911 sodium silicate Inorganic materials 0.000 description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 229960004887 ferric hydroxide Drugs 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 229910052770 Uranium Inorganic materials 0.000 description 4
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 4
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 4
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000011343 solid material Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- IRXRGVFLQOSHOH-UHFFFAOYSA-L dipotassium;oxalate Chemical compound [K+].[K+].[O-]C(=O)C([O-])=O IRXRGVFLQOSHOH-UHFFFAOYSA-L 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 150000004679 hydroxides Chemical class 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910001854 alkali hydroxide Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012612 commercial material Substances 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 238000003891 environmental analysis Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000003295 industrial effluent Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 238000005325 percolation Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
- C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
- C22B60/0217—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
- C22B60/0252—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries
- C22B60/0265—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries extraction by solid resins
- C22B60/0273—Extraction by titanium containing adsorbents, e.g. by hydrous titanium oxide
Definitions
- the present invention relates to a process for the preparation of adsorbent materials which can be used for the treatment or analysis of liquids.
- adsorbent materials comprising an inorganic support in which an adsorbent substance is included.
- these adsorbent materials poses certain problems when it is desired to obtain them in the form of a solid phase of selected particle size retaining all the properties of the adsorbent substance and moreover having satisfactory mechanical characteristics and good resistance to chemical agents.
- the mineral compounds used are generally sodium silicate (US-A-2,057,414) or mixtures of sodium silicate and other compounds such as ferrous oxide (FR-A-941,035), zinc oxide (GB-A-521 214), or calcium aluminate (US-A-2 914 487).
- the present invention specifically relates to a process for preparing an adsorbent material comprising an inorganic support in which is included an adsorbent substance, which makes it possible to obtain materials of high porosity having a high content of adsorbent substance and which also has the advantage of being simple and of low cost, and of requiring only very few additional operations to transform the solid material obtained into a powder of desired particle size.
- the process according to the invention for preparing an adsorbent material is characterized in that it consists in preparing an aqueous solution of an alkali metal silicate and of a compound chosen from the group comprising the hydroxides of alkali metals and ammonia, mixing said solution with an adsorbent substance in the form of powder or gel, and subjecting the mixture thus obtained to a heat treatment.
- an aqueous solution containing an alkali metal hydroxide or ammonia a material of high porosity is obtained by the process of the invention.
- the addition to the aqueous solution of alkali metal silicate of an alkali metal hydroxide or of ammonia makes it possible to obtain a clearly basic pH and this plays a primordial role in favoring during the subsequent phases of heating and desiccation the formation of a crystalline organization of great porosity.
- the method of the invention also has the advantage of simply requiring a heat treatment to directly obtain a mineral support in which an adsorbent substance is included.
- adsorbent materials having a high content of adsorbent substance for example from 70 to 80% by weight of adsorbent substance, which n This is not the case with the methods of the prior art in which the adsorbent substance is fixed on a solid support by impregnation.
- the aqueous starting solution consists of a solution of an alkali metal silicate and hydroxide of the same alkali metal.
- silicate and sodium hydroxide are used.
- the adsorbent substance used can be acidic, neutral or basic.
- adsorbent substances capable of being used there may be mentioned as non-limiting oxides or hydroxides of iron, manganese, titanium, zirconium ...
- the adsorbent substance is titanium hydroxide, ferric hydroxide or manganese oxide.
- titanium hydroxide When using titanium hydroxide, it is preferably added to the aqueous solution in the form of a gel which can, for example, be obtained by adding sodium hydroxide to a solution of titanyl potassium oxalate followed flocculation of the colloidal precipitate thus obtained.
- ferric hydroxide When using ferric hydroxide, it is added in the form of flocs obtained by neutralization of a solution of ferric chloride.
- manganese oxide When manganese oxide is used, it is generally added to the solution as a powder of MnO z .
- the heat treatment is preferably carried out in at least two stages carried out at different temperatures, at least a first stage at a temperature below 100 ° C and a second stage at a temperature from 100 ° C to 400 ° vs.
- the heat treatment is carried out in two stages carried out at different temperatures, the first stage being carried out at a temperature lower than 100 ° C for approximately one day, the second stage being carried out at a temperature higher than 100 ° C and lower than 400 ° C for a few hours to obtain a product whose weight remains constant.
- the heat treatment is advantageously carried out in three stages, the first stage being carried out at approximately 60 ° C for approximately 20 h, the second stage at approximately 90 ° C for approximately 6 h and the third stage at approximately 180 ° C to obtain a constant weight.
- a porous adsorbent material is obtained having a specific surface of at least 200 m 2 / g (hot BET method).
- the adsorbent materials thus obtained can be used as such in the form of a porous percolation structure, or be transformed into grains whose dimensions are adjusted according to the use, by simple grinding and sieving operations.
- the adsorbent material obtained is subjected to washing to remove the excess hydroxide.
- the invention also relates to an adsorbent material usable for the treatment or analysis of liquids containing organic or mineral materials.
- This material is characterized in that it has a specific surface at least equal to 200 m 2 / g and in that it comprises an inorganic support constituted by the product of the reaction of an alkali metal silicate and a hydroxide of the same alkali metal, and an adsorbent substance included in said support.
- the alkali metal is sodium.
- the adsorbent substance is titanium hydroxide, ferric hydroxide or manganese oxide.
- the adsorbent material comprises from 70 to 80% by weight of adsorbent substance.
- the adsorbent materials according to the invention can be used for the extraction of mineral or organic compounds during the treatment of industrial effluents, radioactive or not, as well as for measurements relating to environmental pollution.
- such adsorbent materials containing titanium hydroxide can be used to recover uranium from aqueous solutions such as mine water.
- This example relates to the preparation of an adsorbent material consisting of an inorganic support made of silicate and sodium hydroxide in which is included titanium hydroxide.
- a solution of silicate and sodium hydroxide is prepared by mixing 38 ml of a technical sodium silicate solution Si0 3 Na 2 having a density of 1.33 to 1.34 with 13 ml of a sodium hydroxide solution having a density of 1.32.
- a titanium hydroxide gel is prepared from a solution of titanyl potassium oxalate in distilled water. This solution is brought to pH 6.5-6.8 by addition of sodium hydroxide, then the colloidal precipitate thus obtained is flocculated by means of an anionic flocculant sold under the brand Magnafloc to facilitate its filtration. After flocculation and filtration, a titanium hydroxide gel is obtained, the water content of which is approximately 90%.
- the solid adsorbent material obtained after heat treatment has a specific surface of 200 m 2 / g, a titanium hydroxide content of 73% and a pore volume of 1030 mm 3. g- 1.
- This material is transformed into grains by grinding and sieving, at a particle size of between 0.5 and 2 mm, with a view to being used for the extraction of uranium from mine mine water in the following manner.
- an adsorbent material is obtained having the same characteristics.
- This example relates to the preparation of adsorbent material containing as adsorbent substance ferric hydroxide Fe (OH) 3 .
- a solution of silicate and sodium hydroxide is prepared, as in Example 1, using the same quantities of products.
- ferric hydroxide gel Fe (OH) s is prepared by neutralization at pH 7 of a solution of ferric chloride.
- the solid adsorbent material obtained after this heat treatment has a specific surface of 214 m 2 / g.
- ferric hydroxide Fe (OH) 3 has only a specific surface of 158 m Z / g.
- the process of the invention makes it possible to obtain a significant improvement in the porosity of the material obtained.
- This example relates to the preparation of an adsorbent material containing Mn0 2 as an adsorbent substance.
- a solution of silicate and sodium hydroxide is prepared by mixing 40 ml of a technical sodium silicate solution Si0 3 Na z having a density of 1.33 to 1.34 with 20 ml of a NaOH solution with 32%.
- the solid adsorbent material obtained after this heat treatment has a specific surface of 201 m Z / g.
- the commercial product currently sold which also contains manganese dioxide, has a specific surface of 124 m 2 / g.
- This example relates to the preparation of an adsorbent material consisting of a sodium silicate support in which is included titanium hydroxide.
- the adsorbent material is prepared by adding 500 g of titanium hydroxide gel prepared in the same way as in Example 1 to 38 ml of a solution of technical sodium silicate Si0 3 Naz having a density of 1.33 to 1.34, and the whole is thoroughly mixed which is then subjected to heat treatment carried out under the same conditions as those of Example 1.
- the adsorbent material thus obtained has a specific surface of 165 ⁇ 5 m 2 / g.
- Example 1 which starts with a solution of silicate and sodium hydroxide, it can be seen that the addition of soda to the starting solution makes it possible to obtain a significant improvement in the specific surface of the adsorbent material obtained.
- This example illustrates the influence of the temperature used in the last stage of the heat treatment on the specific surface of the adsorbent material obtained.
- a mixture of silicate solution is prepared in the same way as in Example 1 and of sodium hydroxide and of titanium hydroxide gel, then this mixture is subjected to a heat treatment carried out under the same conditions as those of Example 1 for the first two stages, and the third stage is carried out either at a temperature 100 ° C, or at a temperature of 440 ° C, until a constant weight is obtained.
- the solid adsorbent material obtained after this heat treatment has a specific surface of 135 m 2 fg when the last step is carried out at 100 ° C and a specific surface of 180 m z / g when the last step is carried out at 440 ° C.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Inorganic Chemistry (AREA)
- Geology (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR8007460 | 1980-04-02 | ||
| FR8007460A FR2479986A1 (fr) | 1980-04-02 | 1980-04-02 | Procede de preparation de materiaux adsorbants destines a l'analyse ou au traitement des liquides et les materiaux ainsi obtenus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0037321A1 EP0037321A1 (fr) | 1981-10-07 |
| EP0037321B1 true EP0037321B1 (fr) | 1984-03-14 |
Family
ID=9240468
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP81400456A Expired EP0037321B1 (fr) | 1980-04-02 | 1981-03-23 | Procédé de préparation de matériaux adsorbants destinés à l'analyse ou au traitement des liquides et les matériaux ainsi obtenus |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US4366090A (https=) |
| EP (1) | EP0037321B1 (https=) |
| JP (1) | JPS56155643A (https=) |
| CA (1) | CA1171839A (https=) |
| DE (1) | DE3162576D1 (https=) |
| ES (1) | ES500985A0 (https=) |
| FR (1) | FR2479986A1 (https=) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4591581A (en) * | 1983-01-28 | 1986-05-27 | Laporte Industries Limited | Method for making absorbent materials |
| IT1223582B (it) * | 1987-12-22 | 1990-09-29 | Eniricerche Spa | Procedimento per la preparazione di dispersioni solide di sali acidi di metalli tetravalenti a struttura lamellare inuna matrice inorganica inerte e prodotti cosi' ottenuti |
| US20020074292A1 (en) * | 2000-09-26 | 2002-06-20 | Andreas Schlegel | Adsorption vessels |
| AU2002218168A1 (en) * | 2000-09-26 | 2002-04-08 | Bayer Aktiengesellschaft | Contact and adsorber granulates |
| BR0114198B1 (pt) * | 2000-09-26 | 2012-02-22 | unidades de filtração percorrìveis por meios para remoção de substáncias nocivas de lìquidos. | |
| WO2002026631A1 (de) * | 2000-09-26 | 2002-04-04 | Bayer Aktiengesellschaft | Kontakt- und adsorber-granulate |
| DE10116953B4 (de) * | 2001-04-05 | 2010-04-29 | Wismut Gmbh | Verfahren zur Abtrennung von Schwermetallen, Metallen, Arsen, Uran und Radium aus schadstoffbelasteten Wässern durch ein aus mehreren Komponenten bestehendes reaktives Material |
Family Cites Families (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB289890A (https=) * | 1927-05-06 | 1929-08-06 | The Silica Gel Corporation | |
| GB392954A (en) * | 1930-11-21 | 1933-05-22 | Silica Gel Corp | Improvements in or relating to catalytic or adscrption processes and the manufactureof plural or mixed gels therefor |
| US1999210A (en) * | 1931-04-10 | 1935-04-30 | Johns Manville | Hydrous silicate gels and method of making the same |
| DE745752C (de) * | 1933-07-16 | 1944-05-05 | Ig Farbenindustrie Ag | Herstellung poroeser, insbesondere fuer Adsorptions- oder katalytische Zwecke geeigneter aktiver Massen |
| US2057414A (en) * | 1935-03-28 | 1936-10-13 | Southwick W Briggs | Oil filtering element and process of making the same |
| GB521214A (en) * | 1938-09-21 | 1940-05-15 | Herbert Hans Greger | Improvements in or relating to bonding fuller's earth or other absorbent granular material |
| US2265389A (en) * | 1939-02-07 | 1941-12-09 | Standard Oil Co | Catalytic cracking process |
| FR941035A (fr) * | 1940-11-19 | 1948-12-30 | Procédé de fabrication d'une matière absorbante et composition réalisée par ce procédé | |
| US2407247A (en) * | 1940-11-19 | 1946-09-10 | Southwick W Briggs | Bonded adsorbent |
| US2344911A (en) * | 1942-03-28 | 1944-03-21 | Standard Oil Dev Co | Titanium catalyst |
| US2699376A (en) * | 1950-08-01 | 1955-01-11 | Gulf Research Development Co | Process for increasing the a verage pore size of a calcined silica gel |
| US2914487A (en) * | 1955-06-15 | 1959-11-24 | Sporlan Valve Company Inc | Bonding of adsorbent materials |
| FR1537777A (fr) * | 1967-07-04 | 1968-08-30 | Pechiney Saint Gobain | Particules sphéroïdales d'hydroxydes |
| US3775345A (en) * | 1971-05-28 | 1973-11-27 | Grace W R & Co | Amorphous inorganic gel |
-
1980
- 1980-04-02 FR FR8007460A patent/FR2479986A1/fr active Granted
-
1981
- 1981-03-23 DE DE8181400456T patent/DE3162576D1/de not_active Expired
- 1981-03-23 EP EP81400456A patent/EP0037321B1/fr not_active Expired
- 1981-03-24 US US06/247,201 patent/US4366090A/en not_active Expired - Fee Related
- 1981-04-01 ES ES500985A patent/ES500985A0/es active Granted
- 1981-04-01 JP JP4924981A patent/JPS56155643A/ja active Pending
- 1981-04-01 CA CA000374421A patent/CA1171839A/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CA1171839A (en) | 1984-07-31 |
| DE3162576D1 (en) | 1984-04-19 |
| US4366090A (en) | 1982-12-28 |
| FR2479986A1 (fr) | 1981-10-09 |
| FR2479986B1 (https=) | 1984-04-13 |
| EP0037321A1 (fr) | 1981-10-07 |
| ES8202153A1 (es) | 1982-01-01 |
| ES500985A0 (es) | 1982-01-01 |
| JPS56155643A (en) | 1981-12-01 |
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